CN114000349A - Alginate-encapsulated bacterial cellulose composite photo-thermal antibacterial medical dressing and preparation method thereof - Google Patents
Alginate-encapsulated bacterial cellulose composite photo-thermal antibacterial medical dressing and preparation method thereof Download PDFInfo
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- CN114000349A CN114000349A CN202111486894.6A CN202111486894A CN114000349A CN 114000349 A CN114000349 A CN 114000349A CN 202111486894 A CN202111486894 A CN 202111486894A CN 114000349 A CN114000349 A CN 114000349A
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- Prior art keywords
- nano
- bacterial cellulose
- composite
- alginate
- solution
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- 229920002749 Bacterial cellulose Polymers 0.000 title claims abstract description 161
- 239000005016 bacterial cellulose Substances 0.000 title claims abstract description 161
- 239000002131 composite material Substances 0.000 title claims abstract description 160
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 235000010443 alginic acid Nutrition 0.000 claims abstract description 23
- 229920000615 alginic acid Polymers 0.000 claims abstract description 23
- 206010052428 Wound Diseases 0.000 claims abstract description 10
- 208000027418 Wounds and injury Diseases 0.000 claims abstract description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 157
- 239000000243 solution Substances 0.000 claims description 122
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims description 81
- 239000011787 zinc oxide Substances 0.000 claims description 74
- 239000007788 liquid Substances 0.000 claims description 57
- 239000002608 ionic liquid Substances 0.000 claims description 46
- 210000004379 membrane Anatomy 0.000 claims description 46
- 239000012528 membrane Substances 0.000 claims description 46
- 238000009987 spinning Methods 0.000 claims description 45
- 229920002678 cellulose Polymers 0.000 claims description 41
- 239000001913 cellulose Substances 0.000 claims description 41
- 238000010041 electrostatic spinning Methods 0.000 claims description 39
- 239000006185 dispersion Substances 0.000 claims description 37
- 238000002156 mixing Methods 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 238000001035 drying Methods 0.000 claims description 27
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 239000000661 sodium alginate Substances 0.000 claims description 24
- 235000010413 sodium alginate Nutrition 0.000 claims description 24
- 229940005550 sodium alginate Drugs 0.000 claims description 24
- 238000002791 soaking Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 18
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 16
- 229940072056 alginate Drugs 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 16
- 238000004140 cleaning Methods 0.000 claims description 16
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 12
- 230000001112 coagulating effect Effects 0.000 claims description 11
- 239000002105 nanoparticle Substances 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 150000003839 salts Chemical class 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 7
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 claims description 7
- 239000006184 cosolvent Substances 0.000 claims description 6
- PXKPKGHXANCVMC-UHFFFAOYSA-N 3-butyl-1-methyl-1,2-dihydroimidazol-1-ium;trifluoromethanesulfonate Chemical compound OS(=O)(=O)C(F)(F)F.CCCCN1CN(C)C=C1 PXKPKGHXANCVMC-UHFFFAOYSA-N 0.000 claims description 5
- SFPTVQNKTCPLAX-UHFFFAOYSA-N 3-ethyl-1-methyl-1,2-dihydroimidazol-1-ium;2,2,2-trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F.CC[NH+]1CN(C)C=C1 SFPTVQNKTCPLAX-UHFFFAOYSA-N 0.000 claims description 5
- 150000001768 cations Chemical group 0.000 claims description 5
- ZDIRKWICVFDSNX-UHFFFAOYSA-N diethyl phosphate 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium Chemical compound P(=O)(OCC)(OCC)O.C(C)N1CN(C=C1)C ZDIRKWICVFDSNX-UHFFFAOYSA-N 0.000 claims description 5
- ALGZQMQWKPQOER-UHFFFAOYSA-N 1-butyl-3-methyl-2H-imidazole cyanocyanamide Chemical compound N#CNC#N.CCCCN1CN(C)C=C1 ALGZQMQWKPQOER-UHFFFAOYSA-N 0.000 claims description 4
- ZXLOSLWIGFGPIU-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCN1CN(C)C=C1 ZXLOSLWIGFGPIU-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 229920001046 Nanocellulose Polymers 0.000 claims description 4
- 208000002847 Surgical Wound Diseases 0.000 claims description 4
- -1 1-allyl-3-methylimidazole chloride salt Chemical class 0.000 claims description 3
- IAZSXUOKBPGUMV-UHFFFAOYSA-N 1-butyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CCCC[NH+]1CN(C)C=C1 IAZSXUOKBPGUMV-UHFFFAOYSA-N 0.000 claims description 3
- FQERWQCDIIMLHB-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;chloride Chemical compound [Cl-].CC[NH+]1CN(C)C=C1 FQERWQCDIIMLHB-UHFFFAOYSA-N 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 230000015271 coagulation Effects 0.000 claims description 3
- 238000005345 coagulation Methods 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- 210000002747 omentum Anatomy 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 24
- 150000004781 alginic acids Chemical class 0.000 abstract description 7
- 229960001126 alginic acid Drugs 0.000 abstract description 6
- 239000000783 alginic acid Substances 0.000 abstract description 6
- 230000035699 permeability Effects 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 210000001124 body fluid Anatomy 0.000 abstract description 2
- 239000010839 body fluid Substances 0.000 abstract description 2
- 239000003792 electrolyte Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 230000017423 tissue regeneration Effects 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 238000005303 weighing Methods 0.000 description 12
- 238000005406 washing Methods 0.000 description 9
- 238000004108 freeze drying Methods 0.000 description 7
- 238000000967 suction filtration Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- FHDQNOXQSTVAIC-UHFFFAOYSA-M 1-butyl-3-methylimidazol-3-ium;chloride Chemical compound [Cl-].CCCCN1C=C[N+](C)=C1 FHDQNOXQSTVAIC-UHFFFAOYSA-M 0.000 description 4
- BMQZYMYBQZGEEY-UHFFFAOYSA-M 1-ethyl-3-methylimidazolium chloride Chemical compound [Cl-].CCN1C=C[N+](C)=C1 BMQZYMYBQZGEEY-UHFFFAOYSA-M 0.000 description 4
- QVRCRKLLQYOIKY-UHFFFAOYSA-M 1-methyl-3-prop-2-enylimidazol-1-ium;chloride Chemical compound [Cl-].C[N+]=1C=CN(CC=C)C=1 QVRCRKLLQYOIKY-UHFFFAOYSA-M 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 4
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 4
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 description 4
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Chemical compound [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 description 4
- UBXAKNTVXQMEAG-UHFFFAOYSA-L strontium sulfate Chemical compound [Sr+2].[O-]S([O-])(=O)=O UBXAKNTVXQMEAG-UHFFFAOYSA-L 0.000 description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 description 4
- KAIPKTYOBMEXRR-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole Chemical compound CCCCN1CN(C)C=C1 KAIPKTYOBMEXRR-UHFFFAOYSA-N 0.000 description 3
- 206010016807 Fluid retention Diseases 0.000 description 3
- 230000035876 healing Effects 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 229920001059 synthetic polymer Polymers 0.000 description 3
- ICIVTHOGIQHZRY-UHFFFAOYSA-N 1-butyl-3-methylimidazol-3-ium;cyanoiminomethylideneazanide Chemical compound [N-]=C=NC#N.CCCCN1C=C[N+](C)=C1 ICIVTHOGIQHZRY-UHFFFAOYSA-N 0.000 description 2
- JOKVYNJKBRLDAT-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium;2,2,2-trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F.CC[N+]=1C=CN(C)C=1 JOKVYNJKBRLDAT-UHFFFAOYSA-M 0.000 description 2
- XIYUIMLQTKODPS-UHFFFAOYSA-M 1-ethyl-3-methylimidazol-3-ium;acetate Chemical compound CC([O-])=O.CC[N+]=1C=CN(C)C=1 XIYUIMLQTKODPS-UHFFFAOYSA-M 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- HQWOEDCLDNFWEV-UHFFFAOYSA-M diethyl phosphate;1-ethyl-3-methylimidazol-3-ium Chemical compound CC[N+]=1C=CN(C)C=1.CCOP([O-])(=O)OCC HQWOEDCLDNFWEV-UHFFFAOYSA-M 0.000 description 2
- 208000015181 infectious disease Diseases 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 229910001631 strontium chloride Inorganic materials 0.000 description 2
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical compound [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 2
- 239000011592 zinc chloride Substances 0.000 description 2
- 235000005074 zinc chloride Nutrition 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 description 1
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 description 1
- 102000008186 Collagen Human genes 0.000 description 1
- 108010035532 Collagen Proteins 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 206010072170 Skin wound Diseases 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 241000193996 Streptococcus pyogenes Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229920001586 anionic polysaccharide Polymers 0.000 description 1
- 150000004836 anionic polysaccharides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 230000000740 bleeding effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 230000003013 cytotoxicity Effects 0.000 description 1
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- 230000007423 decrease Effects 0.000 description 1
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- 238000004090 dissolution Methods 0.000 description 1
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- 230000002439 hemostatic effect Effects 0.000 description 1
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- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 description 1
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Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/03—Polysaccharides or derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
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Abstract
The invention discloses an alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing and a preparation method thereof. The composite medical dressing has the biocompatibility, moisture absorption and retention property, excellent mechanical property, antibacterial property, photo-thermal response property and air permeability and oxygen permeability of bacterial cellulose and alginic acid materials, and realizes the free exchange of antibacterial ions and electrolyte in body fluid. The preparation process is controllable, the antibacterial effect is high-efficiency and durable, and the photo-thermal effect is achieved, so that the medical dressing has an important application prospect in the aspects of tissue repair, operation incision and treatment of burn wounds.
Description
Technical Field
The invention belongs to the field of medical composite materials, and particularly relates to alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing and a preparation method thereof.
Background
Skin is the first line of defense of the human body and is also a fragile part of the human body, and the healing of skin wounds is a complex and dynamically changing process, wherein infection is one of the most common factors causing the healing delay of wounds. The wound dressing has the unique advantages of strong pertinence, small side effect and the like in the aspects of diminishing inflammation, stopping bleeding, moisturizing wounds, accelerating healing and the like, and has wide application in a plurality of scenes including surgical wound surfaces. An ideal wound dressing would need to meet the following characteristics simultaneously: porous structure, good mechanical property, high water holding capacity, no toxicity, good histocompatibility and antibacterial activity. Compared with other biomedical materials such as collagen, hyaluronic acid, silica gel and the like, the bacterial cellulose used as a wound repair material has the greatest advantages of extremely high mechanical strength and water retention capacity. However, since the bacterial cellulose itself has no antibacterial function, it is easily contaminated by harmful microorganisms in the air or water, thereby causing a series of infection problems. In order to enable the bacterial cellulose to have an antibacterial function, at present, the bacterial cellulose is usually placed in a bactericide (such as nano-silver) solution in a soaking and adsorbing manner, but the bactericide is low in adsorption efficiency and stability and short in sterilization duration.
Sodium alginate is a natural linear anionic polysaccharide extracted from brown algae, and can form three-dimensional network hydrogel through cationic crosslinking, so that the sodium alginate becomes a wound dressing substrate with excellent biocompatibility. Although cationic crosslinked alginic acids show great potential in the biomedical field, the main problems limiting their use in dressings are the lack of antibacterial activity and poor mechanical properties. It has been reported that the reinforcement of alginic acid materials is achieved by adding a synthetic polymer material, such as polyethylene oxide or polyvinyl alcohol, to sodium alginate, but the addition of a synthetic polymer decreases the histocompatibility of alginic acid materials. In order to solve the problem that the cation cross-linked alginic acid material does not have antibacterial activity, the cation cross-linked alginic acid material can be added with certain antibacterial components (such as nano Ag) to further form cation cross-linked gel to prepare the antibacterial dressing. However, it has been shown that nanoparticles are easily phagocytized by cells and then aggregated in cells, thereby causing cytotoxicity.
How to prepare the biomass medical dressing with porous structure, good mechanical property, high water-holding capacity, no toxicity, good histocompatibility and antibacterial activity on the basis of not introducing synthetic polymer materials is still a difficult problem in scientific research and production practice.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of alginate-encapsulated bacterial cellulose composite photo-thermal antibacterial medical dressing, and the alginate-encapsulated bacterial cellulose composite medical dressing prepared by the method not only keeps the biocompatibility, moisture absorption and water retention of bacterial cellulose and alginic acid materials, but also endows the composite material with excellent mechanical property, antibacterial property and photo-thermal response property. The nanofiber membrane with the porous structure prepared by the electrostatic spinning technology ensures the permeability and oxygen permeability of the dressing and realizes the free exchange of antibacterial zinc ions and electrolyte in body fluid.
In order to achieve the purpose, the invention adopts the technical scheme that:
on one hand, the invention provides a preparation method of alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing, which comprises the following steps:
s1, preparing a bacterial cellulose solution:
crushing a bacterial cellulose omentum by using a mechanical homogenization method to obtain a bacterial cellulose homogenate;
the bacterial cellulose homogenate is put into a sodium hydroxide solution for soaking and purification after centrifugal dewatering, is washed to be neutral, is filtered, frozen and dried to obtain the pretreated bacterial cellulose;
dissolving bacterial cellulose in ionic liquid to obtain a bacterial cellulose solution;
s2, preparing photo-thermal antibacterial nano particle dispersion liquid:
mixing the nano-cellulose and the ionic liquid according to the mass ratio of (1-3) to (30-80) to obtain nano-cellulose-ionic liquid;
respectively dispersing nano zinc oxide and nano copper sulfide in nano cellulose-ionic liquid to obtain nano zinc oxide dispersion liquid and nano copper sulfide dispersion liquid;
wherein the mass ratio of the nanocellulose to the nano zinc oxide and the nano copper sulfide is 1:1-10: 1;
s3, preparing the electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the ratio of nano zinc oxide: mixing the nano copper sulfide in a mass ratio of 6:1-1:1 to obtain a functional particle mixed solution; mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:1-100:5 to form a composite spinning solution for an electrostatic spinning process;
s4, preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous film by an electrostatic spinning method, putting the composite nano porous film into deionized water for cleaning, and drying; and immersing the composite membrane in a sodium alginate aqueous solution, putting the composite membrane immersed in the sodium alginate into a metal salt aqueous solution coagulating bath, taking out the composite membrane, and cleaning the composite membrane with deionized water to obtain the alginate-packaged bacterial cellulose composite photothermal antibacterial medical dressing.
Further, in the S1, the mass concentration of the bacterial cellulose solution is 0.5-3%.
In S2, the concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 0.2-2%.
Further, the ionic liquid is an ionic solvent or a mixed solvent composed of the ionic solvent and a cosolvent.
Further, the ionic liquid comprises one or a combination of more of 1-ethyl-3-methylimidazole chloride salt, 1-allyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole chloride salt, 1-ethyl-3-methylimidazole acetate, 1-butyl-3-methylimidazole trifluoromethanesulfonate, 1-butyl-3-methylimidazole dicyanamide salt, 1-ethyl-3-methylimidazole trifluoroacetate and 1-ethyl-3-methylimidazole diethyl phosphate.
Further, the cosolvent is one or a combination of more of 4-methylmorpholine-N-oxide, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Further, the bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane is prepared by an electrostatic spinning method as follows:
injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 15-30 kV voltage, 3-5 mL/h flow rate and 15-25 cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 30-80 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane.
Further, the mass ratio concentration of the sodium alginate aqueous solution is 0.1-1%. The mass ratio concentration of the metal salt water solution coagulation bath is 1-5%.
Further, the coagulating bath of the metal salt water solution is one or more of hydrochloride, nitrate or sulfate of calcium, strontium, iron, copper or zinc.
On the other hand, the invention provides the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing prepared by the method, the composite photothermal antibacterial medical dressing comprises an inner layer structure and an outer layer structure, the inner layer is a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous film structure, and the outer layer is a cation cross-linked alginate encapsulation structure.
Compared with the prior art, the invention has the following beneficial effects:
the polymer base material of the medical dressing prepared by the invention mainly adopts the raw materials of bacterial cellulose and sodium alginate which are all purely natural biomass high molecular materials, and has excellent biocompatibility. Through the design of the alginate-encapsulated bacterial cellulose/nano zinc oxide/nano copper sulfide composite structure, the hemostatic performance and the ion exchange performance of alginate, the toughness performance and the water retention performance of bacterial cellulose can be effectively exerted. In the internal bacterial cellulose/zinc oxide/copper sulfide composite electrostatic spinning membrane, zinc oxide serving as a zinc source can be pressed into an alginate system through osmotic pressure to convey zinc ions, and further alginate releases zinc ion antibacterial elements to a wound surface through ion exchange, so that a lasting antibacterial effect is achieved. And the existence of the photo-thermal agent copper sulfide can directionally irradiate the medical dressing through infrared light, so that photo-thermal conversion on the dressing is effectively realized, the transmission and release rate of zinc ions are promoted through thermal action, and the intelligent controllability of the antibacterial medical dressing in the treatment process is realized.
The dissolution of the bacterial cellulose, the preparation method of the zinc oxide and copper sulfide nano particle dispersion liquid is simple and easy to implement, the alginate material is uniformly and efficiently packaged on the bacterial cellulose composite film, and the nano porous structure of the bacterial cellulose cannot be damaged; meanwhile, the mechanical property, the water holding capacity and the air permeability of the dressing are ensured, the preparation process is green and environment-friendly, the cost is low, and the industrial production can be realized. The alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing is applied to surgical incisions and burn wounds, and has a good application prospect.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
The invention provides a preparation method of alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing, which comprises the following steps:
step 1, preparing a bacterial cellulose solution:
crushing a bacterial cellulose omentum by using a mechanical homogenization method to obtain a bacterial cellulose homogenate;
centrifuging the bacterial cellulose homogenate to remove water, then putting the homogenate into a sodium hydroxide solution for soaking and purifying, cleaning the homogenate to be neutral, performing suction filtration, and performing freeze drying to obtain pretreated bacterial cellulose;
and (3) dissolving the bacterial cellulose in the ionic liquid to obtain a bacterial cellulose solution with the mass concentration of 0.5-3%.
Wherein the ionic liquid is an ionic solvent or a mixed solvent consisting of the ionic solvent and a cosolvent;
the ionic liquid comprises one or more of 1-ethyl-3-methylimidazole chloride salt, 1-allyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole chloride salt, 1-ethyl-3-methylimidazole acetate, 1-butyl-3-methylimidazole trifluoromethanesulfonate, 1-butyl-3-methylimidazole dicyanamide salt, 1-ethyl-3-methylimidazole trifluoroacetate and 1-ethyl-3-methylimidazole diethyl phosphate.
The cosolvent is one or more of 4-methylmorpholine-N-oxide, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Step 2, preparing photo-thermal antibacterial nano particle dispersion liquid:
mixing the nano-cellulose and the ionic liquid according to the mass ratio of (1-3) to (30-80) to obtain nano-cellulose-ionic liquid; dispersing nano zinc oxide in nano cellulose-ionic liquid according to the mass ratio of 1:1-10:1 of nano cellulose to nano zinc oxide to obtain nano zinc oxide dispersion liquid;
and dispersing the nano copper sulfide in nano cellulose-ionic liquid according to the mass ratio of 1:1-10:1 of the nano cellulose to the nano copper sulfide to obtain nano copper sulfide dispersion liquid.
The concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 0.2 to 2 percent.
Step 3, preparing the electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the weight ratio of nano zinc oxide: mixing the nano copper sulfide in a mass ratio of 6:1-1:1 to obtain a functional particle mixed solution;
and mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:1-100:5 to form the composite spinning solution for the electrostatic spinning process.
Step 4, preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane by an electrostatic spinning method: injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 15-30 kV voltage, 3-5 mL/h flow rate and 15-25 cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 30-80 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite electrostatic spinning film.
Then cleaning the composite nano porous film by using deionized water, and drying; immersing the composite membrane into a sodium alginate aqueous solution with the mass ratio concentration of 0.1-1%, putting the composite membrane immersed with the sodium alginate into a coagulating bath of a metal salt aqueous solution with the mass ratio concentration of 1-5%, taking out the composite membrane and washing the composite membrane with deionized water to obtain the alginate-encapsulated bacterial cellulose composite photo-thermal antibacterial medical dressing.
The coagulating bath of the metal salt aqueous solution is one or more of calcium chloride, strontium chloride, ferric chloride, copper chloride and zinc chloride, or calcium nitrate, strontium nitrate, ferric nitrate, copper nitrate and zinc nitrate, or calcium sulfate, strontium sulfate, ferric sulfate, copper sulfate or zinc sulfate.
The present invention will be described in further detail with reference to specific examples.
Example 1
1) Preparing a bacterial cellulose solution:
1g of bacterial cellulose is dissolved in 1L of deionized water, and the mixture is homogenized in a high-pressure homogenizer for 20 minutes, wherein the homogenizing pressure is set to be 80MPa, so that the bacterial cellulose homogenate is obtained.
And (2) centrifuging the homogenized bacterial cellulose solution in a high-speed centrifuge with the speed of 10000 r/min for 10 min to obtain wet bacterial cellulose, soaking the obtained wet bacterial cellulose in a sodium hydroxide solution with the pH value of 12 for 24 h, performing suction filtration and washing to neutrality, and freeze-drying the obtained purified bacterial cellulose for later use.
Dissolving the obtained dry bacterial cellulose in a 1-ethyl-3-methylimidazolium chloride ionic liquid solvent to prepare a bacterial cellulose ionic liquid solution with the mass fraction of 0.5%.
2) Preparing photo-thermal antibacterial nanoparticle dispersion liquid:
mixing the nano-cellulose and the ionic liquid according to the mass ratio of 1:50 to obtain a nano-cellulose/1-ethyl-3-methylimidazolium chloride ionic liquid solution.
Weighing the materials according to the mass ratio of the nano-cellulose to the nano-zinc oxide of 8:1, and dispersing the nano-zinc oxide in the nano-cellulose/1-ethyl-3-methylimidazolium chloride ionic liquid solution to obtain a nano-zinc oxide dispersion liquid.
Weighing the materials according to the mass ratio of 7:1 of the nano-cellulose to the nano-copper sulfide, and dispersing the nano-copper sulfide in the nano-cellulose/1-ethyl-3-methylimidazolium chloride ionic liquid solution to obtain the nano-copper sulfide dispersion liquid.
The concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 1%.
3) Preparing an electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the weight ratio of nano zinc oxide: mixing the nano copper sulfide with the mass ratio of 6:1 to obtain functional particle mixed solution;
and mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:3 to form the composite spinning solution for the electrostatic spinning process.
4) Preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane by an electrostatic spinning method: injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 20kV voltage, 4mL/h flow rate and 20cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 60 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite electrostatic spinning membrane.
Then cleaning the composite nano porous film by using deionized water, and drying; immersing the composite membrane in a sodium alginate aqueous solution with the mass ratio concentration of 0.5%, putting the composite membrane immersed with the sodium alginate into a calcium chloride coagulating bath with the mass ratio concentration of 3%, taking out the composite membrane and cleaning the composite membrane with deionized water to obtain the alginate-packaged bacterial cellulose composite photothermal antibacterial medical dressing.
Example 2
1) Preparing a bacterial cellulose solution:
1g of bacterial cellulose is dissolved in 1L of deionized water, and the mixture is homogenized in a high-pressure homogenizer for 20 minutes, wherein the homogenizing pressure is set to be 60MPa, so that the bacterial cellulose homogenate is obtained.
And (2) centrifuging the homogenized bacterial cellulose solution in a high-speed centrifuge at 8000 rpm for 10 minutes to obtain wet bacterial cellulose, soaking the obtained wet bacterial cellulose in a sodium hydroxide solution with the pH value of 12 for 24 hours, performing suction filtration and washing to neutrality, and freeze-drying the obtained purified bacterial cellulose for later use.
And dissolving the obtained dry bacterial cellulose in 1-butyl-3-methylimidazolium chloride ionic liquid to prepare a bacterial cellulose ionic liquid solution with the mass fraction of 2%.
2) Preparing photo-thermal antibacterial nanoparticle dispersion liquid:
mixing the nano-cellulose and the ionic liquid according to the mass ratio of 1:30 to obtain a nano-cellulose/1-butyl-3-methylimidazolium chloride ionic liquid solution; weighing the materials according to the mass ratio of the nano-cellulose to the nano-zinc oxide of 9:1, and dispersing the nano-zinc oxide in the nano-cellulose/1-butyl-3-methylimidazolium chloride ionic liquid solution to obtain a nano-zinc oxide dispersion liquid.
Weighing the materials according to the mass ratio of the nano-cellulose to the nano-copper sulfide of 10:1, and dispersing the nano-copper sulfide in the nano-cellulose/1-butyl-3-methylimidazolium chloride ionic liquid solution to obtain a nano-copper sulfide dispersion liquid.
The concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 0.8 percent.
3) Preparing an electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the weight ratio of nano zinc oxide: mixing the nano copper sulfide with the mass ratio of 5:1 to obtain functional particle mixed solution;
and mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:1 to form the composite spinning solution for the electrostatic spinning process.
4) Preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane by an electrostatic spinning method: injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 25kV voltage, 3mL/h flow rate and 25cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 40 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite electrostatic spinning film.
Then cleaning the composite nano porous film by using deionized water, and drying; immersing the composite membrane in 1% sodium alginate aqueous solution, putting the composite membrane in 2% calcium nitrate, copper nitrate and zinc nitrate coagulating bath, taking out, and washing with deionized water to obtain the alginate-packaged bacterial cellulose composite photo-thermal antibacterial medical dressing.
Example 3
1) Preparing a bacterial cellulose solution:
1g of bacterial cellulose is dissolved in 1L of deionized water, and the mixture is homogenized in a high-pressure homogenizer for 20 minutes, wherein the homogenizing pressure is set to be 60MPa, so that the bacterial cellulose homogenate is obtained.
And (2) centrifuging the homogenized bacterial cellulose solution in a high-speed centrifuge at 8000 rpm for 10 minutes to obtain wet bacterial cellulose, soaking the obtained wet bacterial cellulose in a sodium hydroxide solution with the pH value of 12 for 24 hours, performing suction filtration and washing to neutrality, and freeze-drying the obtained purified bacterial cellulose for later use.
Dissolving the obtained dry bacterial cellulose in a composite solvent with the mass ratio of 1:1 of 1-allyl-3-methylimidazolium chloride ionic liquid to 4-methylmorpholine-N-oxide, and preparing a bacterial cellulose ionic liquid solution with the mass fraction of 1.5%.
2) Preparing photo-thermal antibacterial nanoparticle dispersion liquid:
mixing the nano-cellulose and the ionic liquid according to the mass ratio of 1:80 to obtain a nano-cellulose/1-allyl-3-methylimidazolium chloride ionic liquid and a 4-methylmorpholine-N-oxide composite solution; weighing the materials according to the mass ratio of the nano-cellulose to the nano-zinc oxide of 5:1, and dispersing the nano-zinc oxide in the nano-cellulose/1-allyl-3-methylimidazolium chloride ionic liquid and 4-methylmorpholine-N-oxide composite solution to obtain the nano-zinc oxide dispersion solution.
Weighing the materials according to the mass ratio of the nano-cellulose to the nano-copper sulfide of 5:1, and dispersing the nano-copper sulfide in the nano-cellulose/1-allyl-3-methylimidazolium chloride ionic liquid and 4-methylmorpholine-N-oxide composite solution to obtain the nano-copper sulfide dispersion liquid.
The concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 0.2 percent.
3) Preparing an electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the weight ratio of nano zinc oxide: mixing the nano copper sulfide with the mass ratio of 5:1 to obtain functional particle mixed solution;
and mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:2 to form the composite spinning solution for the electrostatic spinning process.
4) Preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane by an electrostatic spinning method: injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 30kV voltage, 3mL/h flow rate and 15cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 30 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite electrostatic spinning membrane.
Then cleaning the composite nano porous film by using deionized water, and drying; immersing the composite membrane dipped with the sodium alginate into a sodium alginate water solution with the mass ratio concentration of 0.1%, putting the composite membrane dipped with the sodium alginate into a strontium sulfate, zinc sulfate and copper sulfate coagulating bath with the mass ratio concentration of 1%, taking out the composite membrane and washing the composite membrane with deionized water to obtain the alginate-packaged bacterial cellulose composite photothermal antibacterial medical dressing.
Example 4
1) Preparing a bacterial cellulose solution:
1g of bacterial cellulose is dissolved in 1L of deionized water, and the mixture is homogenized in a high-pressure homogenizer for 20 minutes, wherein the homogenizing pressure is set to be 60MPa, so that the bacterial cellulose homogenate is obtained.
And (2) centrifuging the homogenized bacterial cellulose solution in a high-speed centrifuge at 8000 rpm for 10 minutes to obtain wet bacterial cellulose, soaking the obtained wet bacterial cellulose in a sodium hydroxide solution with the pH value of 12 for 24 hours, performing suction filtration and washing to neutrality, and freeze-drying the obtained purified bacterial cellulose for later use.
Dissolving the obtained dry bacterial cellulose in a 1-ethyl-3-methylimidazole acetate and 1-ethyl-3-methylimidazole trifluoroacetate + dimethyl sulfoxide composite solvent to prepare a bacterial cellulose ionic liquid solution with the mass fraction of 3%.
2) Preparing photo-thermal antibacterial nanoparticle dispersion liquid:
mixing the nano-cellulose with the ionic liquid according to the mass ratio of 3:50 to obtain a nano-cellulose/1-ethyl-3-methylimidazole acetate and 1-ethyl-3-methylimidazole trifluoroacetate + dimethyl sulfoxide composite solution; weighing the materials according to the mass ratio of 1:1 of the nano-cellulose to the nano-zinc oxide, and dispersing the nano-zinc oxide in a nano-cellulose/1-ethyl-3-methylimidazolium acetate and 1-ethyl-3-methylimidazolium trifluoroacetate + dimethyl sulfoxide composite solution to obtain a nano-zinc oxide dispersion solution.
Weighing the materials according to the mass ratio of 1:1 of the nano-cellulose to the nano-copper sulfide, and dispersing the nano-copper sulfide in a nano-cellulose/1-ethyl-3-methylimidazolium acetate and 1-ethyl-3-methylimidazolium trifluoroacetate + dimethyl sulfoxide composite solution to obtain a nano-copper sulfide dispersion solution.
The concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 1.8 percent.
3) Preparing an electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the weight ratio of nano zinc oxide: mixing the nano copper sulfide in a mass ratio of 1:1 to obtain a functional particle mixed solution;
and mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:5 to form the composite spinning solution for the electrostatic spinning process.
4) Preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane by an electrostatic spinning method: injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 25kV voltage, 5mL/h flow rate and 20cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 80 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite electrostatic spinning membrane.
Then cleaning the composite nano porous film by using deionized water, and drying; immersing the composite membrane in a sodium alginate aqueous solution with the mass ratio concentration of 0.3%, putting the composite membrane immersed with the sodium alginate into a ferric chloride and copper chloride coagulating bath with the mass ratio concentration of 2.5%, taking out and cleaning with deionized water to obtain the alginate-encapsulated bacterial cellulose composite photo-thermal antibacterial medical dressing.
Example 5
1) Preparing a bacterial cellulose solution:
1g of bacterial cellulose is dissolved in 1L of deionized water, and the mixture is homogenized in a high-pressure homogenizer for 20 minutes, wherein the homogenizing pressure is set to be 60MPa, so that the bacterial cellulose homogenate is obtained.
And (2) centrifuging the homogenized bacterial cellulose solution in a high-speed centrifuge at 8000 rpm for 10 minutes to obtain wet bacterial cellulose, soaking the obtained wet bacterial cellulose in a sodium hydroxide solution with the pH value of 12 for 24 hours, performing suction filtration and washing to neutrality, and freeze-drying the obtained purified bacterial cellulose for later use.
Dissolving the obtained dry bacterial cellulose in ionic liquid of a 1-butyl-3-methylimidazole trifluoromethanesulfonate + N, N-dimethylformamide and N, N-dimethylacetamide composite solvent to prepare a bacterial cellulose ionic liquid solution with the mass fraction of 1.2%.
2) Preparing photo-thermal antibacterial nanoparticle dispersion liquid:
mixing the nano-cellulose and the ionic liquid according to the mass ratio of 2:70 to obtain a 1-butyl-3-methylimidazole trifluoromethanesulfonate + N, N-dimethylformamide and N, N-dimethylacetamide composite ionic liquid solution; weighing the materials according to the mass ratio of the nano-cellulose to the nano-zinc oxide of 3:1, and dispersing the nano-zinc oxide in a nano-cellulose/1-butyl-3-methylimidazole trifluoromethanesulfonate + N, N-dimethylformamide and N, N-dimethylacetamide composite solution to obtain a nano-zinc oxide dispersion solution.
Weighing the materials according to the mass ratio of the nano-cellulose to the nano-copper sulfide of 3:1, and dispersing the nano-copper sulfide in a nano-cellulose/1-butyl-3-methylimidazole trifluoromethanesulfonate + N, N-dimethylformamide and N, N-dimethylacetamide composite solution to obtain a nano-copper sulfide dispersion solution.
The concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 2%.
3) Preparing an electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the weight ratio of nano zinc oxide: mixing the nano copper sulfide with the mass ratio of 4:1 to obtain functional particle mixed solution;
and mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:4 to form the composite spinning solution for the electrostatic spinning process.
4) Preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane by an electrostatic spinning method: injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 15kV voltage, 5mL/h flow rate and 22cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 30 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite electrostatic spinning membrane.
Then cleaning the composite nano porous film by using deionized water, and drying; immersing the composite membrane in sodium alginate aqueous solution with mass ratio concentration of 0.6%, putting the composite membrane immersed with the sodium alginate into strontium chloride and zinc chloride coagulating bath with mass ratio concentration of 4%, taking out and cleaning with deionized water to obtain the alginate-packaged bacterial cellulose composite photo-thermal antibacterial medical dressing.
Example 6
1) Preparing a bacterial cellulose solution:
1g of bacterial cellulose is dissolved in 1L of deionized water, and the mixture is homogenized in a high-pressure homogenizer for 20 minutes, wherein the homogenizing pressure is set to be 60MPa, so that the bacterial cellulose homogenate is obtained.
And (2) centrifuging the homogenized bacterial cellulose solution in a high-speed centrifuge at 8000 rpm for 10 minutes to obtain wet bacterial cellulose, soaking the obtained wet bacterial cellulose in a sodium hydroxide solution with the pH value of 12 for 24 hours, performing suction filtration and washing to neutrality, and freeze-drying the obtained purified bacterial cellulose for later use.
Dissolving the obtained dry bacterial cellulose in 1-butyl-3-methylimidazolium dicyanamide salt and 1-ethyl-3-methylimidazolium diethyl phosphate + N-methylpyrrolidone ionic liquid to prepare a bacterial cellulose ionic liquid solution with the mass fraction of 2.5%.
2) Preparing photo-thermal antibacterial nanoparticle dispersion liquid:
mixing the nano-cellulose and the ionic liquid according to the mass ratio of 3:80 to obtain a nano-cellulose/1-butyl-3-methylimidazole dicyanamide salt and 1-ethyl-3-methylimidazole diethyl phosphate + N-methylpyrrolidone composite solution; weighing the materials according to the mass ratio of the nano-cellulose to the nano-zinc oxide of 6:1, and dispersing the nano-zinc oxide in a composite solution of the nano-cellulose 1-butyl-3-methylimidazole dicyanamide salt and 1-ethyl-3-methylimidazole diethyl phosphate salt and N-methylpyrrolidone to obtain a nano-zinc oxide dispersion solution.
Weighing the materials according to the mass ratio of the nano-cellulose to the nano-copper sulfide of 6:1, and dispersing the nano-copper sulfide in a nano-cellulose/1-butyl-3-methylimidazolium dicyanamide salt and 1-ethyl-3-methylimidazolium diethyl phosphate + N-methylpyrrolidone composite solution to obtain a nano-copper sulfide dispersion solution.
The concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 1.5 percent.
3) Preparing an electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the weight ratio of nano zinc oxide: mixing the nano copper sulfide with the mass ratio of 3:1 to obtain functional particle mixed solution;
and mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:5 to form the composite spinning solution for the electrostatic spinning process.
4) Preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane by an electrostatic spinning method: injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 15kV voltage, 4mL/h flow rate and 18cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 50 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite electrostatic spinning membrane.
Then cleaning the composite nano porous film by using deionized water, and drying; immersing the composite membrane in sodium alginate aqueous solution with mass ratio concentration of 0.8%, putting the composite membrane immersed with the sodium alginate into strontium nitrate and ferric nitrate coagulating bath with mass ratio concentration of 5%, taking out and cleaning with deionized water to obtain the alginate-packaged bacterial cellulose composite photo-thermal antibacterial medical dressing.
Comparative example 1
0.1g of micron zinc oxide and 100mL of nano-cellulose/PVA composite aqueous solution with the solid content of 3%, wherein the mass ratio of the nano-cellulose to the PVA in the solution is 3:1, and the composite solution is spread in a watch glass and then naturally dried to prepare the nano-cellulose/PVA/zinc oxide composite antibacterial dressing.
After the antibacterial medical dressings obtained in the above examples and comparative examples are sterilized by Co-60 gamma ray radiation, relevant performance tests are carried out, and the specific test contents and material performances are shown in the following table:
TABLE 1 comparison of the properties of the examples and comparative examples
As can be seen from Table 1, the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing prepared by the invention is far superior to comparative examples in mechanical properties, water absorption properties, antibacterial effect and slow release effect. Wherein the highest wet and dry tensile strengths are 2.3 and 19MPa, respectively, and the wet and dry tensile strengths of the samples of the examples are not less than 1.9 and 16MPa, respectively; the water absorption rate is higher than 600%, the inhibition rate on staphylococcus aureus is higher than 98%, the inhibition rate on escherichia coli is not lower than 97.5%, and the inhibition rate on streptococcus pyogenes is not lower than 96%. The electrostatic spinning structure based on the internal bacterial cellulose/zinc oxide/copper sulfide composite material is combined with the external alginate packaging structure, so that a good slow-release effect and a good photo-thermal characteristic are provided for the medical dressing. Based on the advantages, the medical dressing has important application prospect in the aspects of tissue repair, surgical incision and treatment of burn wound.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (10)
1. A preparation method of alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing is characterized by comprising the following steps:
s1, preparing a bacterial cellulose solution:
crushing a bacterial cellulose omentum by using a mechanical homogenization method to obtain a bacterial cellulose homogenate;
the bacterial cellulose homogenate is put into a sodium hydroxide solution for soaking and purification after centrifugal dewatering, is washed to be neutral, is filtered, frozen and dried to obtain the pretreated bacterial cellulose;
dissolving bacterial cellulose in ionic liquid to obtain a bacterial cellulose solution;
s2, preparing photo-thermal antibacterial nano particle dispersion liquid:
mixing the nano-cellulose and the ionic liquid according to the mass ratio of (1-3) to (30-80) to obtain nano-cellulose-ionic liquid;
respectively dispersing nano zinc oxide and nano copper sulfide in nano cellulose-ionic liquid to obtain nano zinc oxide dispersion liquid and nano copper sulfide dispersion liquid;
wherein the mass ratio of the nanocellulose to the nano zinc oxide and the nano copper sulfide is 1:1-10: 1;
s3, preparing the electrostatic spinning composite spinning solution:
and (3) mixing the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid according to the weight ratio of nano zinc oxide: mixing the nano copper sulfide in a mass ratio of 6:1-1:1 to obtain a functional particle mixed solution; mixing the bacterial cellulose solution and the functional particle mixed solution according to the mass ratio of the bacterial cellulose to the nano zinc oxide to the nano copper sulfide of 100:1-100:5 to form a composite spinning solution for an electrostatic spinning process;
s4, preparing an alginate outer layer coating structure:
preparing a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous film by an electrostatic spinning method, cleaning the composite nano porous film by deionized water, and drying; and immersing the composite membrane in a sodium alginate aqueous solution, putting the composite membrane immersed in the sodium alginate into a metal salt aqueous solution coagulating bath, taking out the composite membrane, and cleaning the composite membrane with deionized water to obtain the alginate-packaged bacterial cellulose composite photothermal antibacterial medical dressing.
2. The preparation method of the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing according to claim 1, wherein the mass concentration of the bacterial cellulose solution is 0.5-3%;
the concentrations of the nano zinc oxide particles and the nano copper sulfide particles in the nano zinc oxide dispersion liquid and the nano copper sulfide dispersion liquid are both 0.2 to 2 percent.
3. The preparation method of the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing as claimed in claim 1, wherein the ionic liquid is an ionic solvent or a mixed solvent composed of an ionic solvent and a cosolvent.
4. The method for preparing the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing according to claim 4, wherein the ionic liquid comprises one or more of 1-ethyl-3-methylimidazole chloride salt, 1-allyl-3-methylimidazole chloride salt, 1-butyl-3-methylimidazole chloride salt, 1-ethyl-3-methylimidazole acetate, 1-butyl-3-methylimidazole trifluoromethanesulfonate, 1-butyl-3-methylimidazole dicyanamide salt, 1-ethyl-3-methylimidazole trifluoroacetate salt and 1-ethyl-3-methylimidazole diethyl phosphate salt.
5. The preparation method of the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing according to claim 4, wherein the cosolvent is one or a combination of more of 4-methylmorpholine-N-oxide, dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
6. The preparation method of the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing as claimed in claim 1, wherein the bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane is prepared by an electrostatic spinning method, and the process is as follows:
injecting the composite spinning solution into an injector, spraying the composite spinning solution on a receiving plate under the conditions of 15-30 kV voltage, 3-5 mL/h flow rate and 15-25 cm receiving distance, soaking the receiving plate sprayed with the composite spinning solution and formed in ethanol for 24 hours, and drying at the drying temperature of 30-80 ℃ to obtain the bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous membrane.
7. The preparation method of the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing according to claim 1, wherein the mass ratio concentration of the sodium alginate aqueous solution is 0.1-1%;
the mass ratio concentration of the metal salt water solution coagulation bath is 1-5%.
8. The preparation method of the alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing as claimed in claim 1, wherein the metal salt aqueous solution coagulation bath is one or more of hydrochloride, nitrate or sulfate of calcium, strontium, iron, copper or zinc.
9. The alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing prepared by the method of any one of claims 1 to 8, which is characterized by comprising an inner layer and an outer layer, wherein the inner layer is a bacterial cellulose/nano zinc oxide/nano copper sulfide composite nano porous film structure, and the outer layer is a cation cross-linked alginate encapsulating structure.
10. The alginate-encapsulated bacterial cellulose composite photothermal antibacterial medical dressing prepared by the method of any one of claims 1-8 is applied to surgical incisions and burn wounds.
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| CN116376076A (en) * | 2023-03-27 | 2023-07-04 | 西安工程大学 | Copper alginate encapsulated bacterial cellulose/nano silver composite antibacterial film, preparation and application |
| CN117503984A (en) * | 2024-01-05 | 2024-02-06 | 浙江百迪生物科技有限公司 | Platelet-rich plasma-copper sulfide composite nanofiber dressing and preparation method thereof |
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